#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/63/4316361.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4316361
loop_
_publ_author_name
'Tian-Wei Wang'
'Jun Wang'
'Shin-ichi Ohkoshi'
'You Song'
'Xiao-Zeng You'
_publ_section_title
;
 Manganese(II)-Octacyanometallate(V) Bimetallic Ferrimagnets with Tc from
 41 to 53 K Obtained in Acidic Media
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7756
_journal_page_last               7763
_journal_paper_doi               10.1021/ic100591h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'32(C H0.25 Mn0.22 N O0.13 W0.13), 2(C H O3), 4(H2 O), 4.03(H)'
_chemical_formula_sum            'C34 H22 Mn7 N32 O14 W4'
_chemical_formula_weight         2222.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   7.6047(6)
_cell_length_b                   7.6047(6)
_cell_length_c                   28.901(4)
_cell_measurement_reflns_used    371
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.76
_cell_volume                     1671.4(3)
_computing_cell_refinement       'SMART '
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            1614
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    8.198
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; bruker, 2000'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1033
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.8800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                555
_reflns_number_total             651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100591h_si_002_1.cif
_cod_data_source_block           complex_1
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_original_sg_symbol_H-M      'I 4/m m m '
_cod_database_code               4316361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8069(6) 0.8069(6) 0.1584(2) 0.0372(14) Uani 1 2 d S . .
C2 C 0.8035(13) 1.0000 0.0821(3) 0.041(2) Uani 0.75 2 d SP . .
C3 C 1.0000 1.0000 0.2118(4) 0.032(2) Uani 1 8 d S . .
C4 C 0.313(3) 0.687(3) 0.0000 0.030(7) Uani 0.25 4 d SP . .
H4A H 0.2266 0.7734 0.0000 0.035 Uiso 0.25 4 calc SPR A 1
Mn1 Mn 0.5000 1.0000 0.0000 0.0397(6) Uani 0.75 8 d SP . .
Mn2 Mn 1.0000 1.0000 0.32636(7) 0.0353(5) Uani 1 8 d S . .
N1 N 0.7056(5) 0.7056(5) 0.16767(19) 0.0411(12) Uani 1 2 d S . .
N2 N 0.6891(11) 1.0000 0.0566(3) 0.050(2) Uani 0.75 2 d SP B .
N3 N 1.0000 1.0000 0.2504(4) 0.039(3) Uani 1 8 d S . .
O1 O 0.5000 0.695(3) 0.0000 0.043(5) Uani 0.50 4 d SP B 1
O1W O 1.0000 1.0000 0.4067(3) 0.054(3) Uani 1 8 d S . .
H1X H 1.0745 1.0745 0.4165 0.065 Uiso 0.25 2 d SPR . .
H1Y H 0.8982 1.0273 0.4165 0.065 Uiso 0.124 1 d PR . .
O2W O 0.5000 0.758(4) 0.0000 0.035(10) Uani 0.25 4 d SP B 2
H2X H 0.5513 0.7180 0.0239 0.042 Uiso 0.0625 1 d PR B 2
H2Y H 0.5513 0.7180 -0.0239 0.042 Uiso 0.0625 1 d PR B 2
O3W O 0.5000 0.0000 0.2500 0.047(2) Uani 1 8 d S . .
H3X H 0.5913 0.0163 0.2664 0.071 Uiso 0.125 1 d PR . .
H3Y H 0.4087 0.0163 0.2664 0.071 Uiso 0.125 1 d PR . .
W1 W 1.0000 1.0000 0.136763(19) 0.0393(2) Uani 1 8 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 W1 177.1(6) . . ?
N2 C2 W1 173.7(9) . . ?
N3 C3 W1 180.000(1) . . ?
O1 C4 O1 95(3) . 2_655 ?
O1 C4 H4A 132.6 . . ?
O1 C4 H4A 132.6 2_655 . ?
O2W C4 H4A 114.2 2_655 . ?
O2W Mn1 O2W 180.000(2) 17_675 . ?
O2W Mn1 N2 90.000(2) 17_675 . ?
O2W Mn1 N2 90.000(3) . . ?
O2W Mn1 N2 90.000(2) 17_675 17_675 ?
O2W Mn1 N2 90.000(3) . 17_675 ?
N2 Mn1 N2 180.0(3) . 17_675 ?
O2W Mn1 N2 90.000(3) 17_675 19 ?
O2W Mn1 N2 90.000(2) . 19 ?
N2 Mn1 N2 97.3(5) . 19 ?
N2 Mn1 N2 82.7(5) 17_675 19 ?
O2W Mn1 N2 90.000(3) 17_675 3_675 ?
O2W Mn1 N2 90.000(2) . 3_675 ?
N2 Mn1 N2 82.7(5) . 3_675 ?
N2 Mn1 N2 97.3(5) 17_675 3_675 ?
N2 Mn1 N2 180.0(3) 19 3_675 ?
O2W Mn1 O1 180.000(5) 17_675 . ?
O2W Mn1 O1 0.000(2) . . ?
N2 Mn1 O1 90.000(1) . . ?
N2 Mn1 O1 90.000(1) 17_675 . ?
N2 Mn1 O1 90.000(1) 19 . ?
N2 Mn1 O1 90.000(1) 3_675 . ?
O2W Mn1 O1 0.000(4) 17_675 17_675 ?
O2W Mn1 O1 180.000(4) . 17_675 ?
N2 Mn1 O1 90.000(1) . 17_675 ?
N2 Mn1 O1 90.000(1) 17_675 17_675 ?
N2 Mn1 O1 90.000(1) 19 17_675 ?
N2 Mn1 O1 90.000(1) 3_675 17_675 ?
O1 Mn1 O1 180.000(2) . 17_675 ?
N3 Mn2 N1 94.46(16) . 27 ?
N3 Mn2 N1 94.46(16) . 25_665 ?
N1 Mn2 N1 171.1(3) 27 25_665 ?
N3 Mn2 N1 94.46(16) . 26_565 ?
N1 Mn2 N1 89.65(3) 27 26_565 ?
N1 Mn2 N1 89.65(3) 25_665 26_565 ?
N3 Mn2 N1 94.46(16) . 28_655 ?
N1 Mn2 N1 89.65(3) 27 28_655 ?
N1 Mn2 N1 89.65(3) 25_665 28_655 ?
N1 Mn2 N1 171.1(3) 26_565 28_655 ?
N3 Mn2 O1W 180.000(1) . . ?
N1 Mn2 O1W 85.54(16) 27 . ?
N1 Mn2 O1W 85.54(16) 25_665 . ?
N1 Mn2 O1W 85.54(16) 26_565 . ?
N1 Mn2 O1W 85.54(16) 28_655 . ?
C1 N1 Mn2 170.6(6) . 25_665 ?
C2 N2 Mn1 171.6(8) . . ?
C3 N3 Mn2 180.000(1) . . ?
C4 O1 C4 175(3) 18_565 . ?
C4 O1 Mn1 92.4(13) 18_565 . ?
C4 O1 Mn1 92.4(13) . . ?
C4 O1 H2X 62.0 18_565 . ?
C4 O1 H2X 119.2 . . ?
Mn1 O1 H2X 77.5 . . ?
C4 O1 H2Y 62.0 18_565 . ?
C4 O1 H2Y 119.2 . . ?
Mn1 O1 H2Y 77.5 . . ?
H2X O1 H2Y 116.5 . . ?
Mn2 O1W H1X 109.5 . . ?
Mn2 O1W H1Y 109.5 . . ?
H1X O1W H1Y 109.5 . . ?
C4 O2W Mn1 110.8(15) 18_565 . ?
C4 O2W H2X 56.2 18_565 . ?
Mn1 O2W H2X 110.9 . . ?
C4 O2W H2Y 56.2 18_565 . ?
Mn1 O2W H2Y 110.9 . . ?
H2X O2W H2Y 108.9 . . ?
H3X O3W H3Y 109.5 . . ?
C1 W1 C1 146.5(3) 3_775 . ?
C1 W1 C1 85.24(9) 3_775 2_755 ?
C1 W1 C1 85.24(9) . 2_755 ?
C1 W1 C1 85.24(9) 3_775 4_575 ?
C1 W1 C1 85.24(9) . 4_575 ?
C1 W1 C1 146.5(3) 2_755 4_575 ?
C1 W1 C3 73.25(17) 3_775 . ?
C1 W1 C3 73.25(17) . . ?
C1 W1 C3 73.25(17) 2_755 . ?
C1 W1 C3 73.25(17) 4_575 . ?
C1 W1 C2 132.42(17) 3_775 2_755 ?
C1 W1 C2 75.2(2) . 2_755 ?
C1 W1 C2 75.2(2) 2_755 2_755 ?
C1 W1 C2 132.42(17) 4_575 2_755 ?
C3 W1 C2 136.6(3) . 2_755 ?
C1 W1 C2 132.42(16) 3_775 . ?
C1 W1 C2 75.2(2) . . ?
C1 W1 C2 132.42(16) 2_755 . ?
C1 W1 C2 75.2(2) 4_575 . ?
C3 W1 C2 136.6(3) . . ?
C2 W1 C2 58.1(3) 2_755 . ?
C1 W1 C2 75.2(2) 3_775 3_775 ?
C1 W1 C2 132.42(16) . 3_775 ?
C1 W1 C2 75.2(2) 2_755 3_775 ?
C1 W1 C2 132.42(16) 4_575 3_775 ?
C3 W1 C2 136.6(3) . 3_775 ?
C2 W1 C2 58.1(3) 2_755 3_775 ?
C2 W1 C2 86.8(5) . 3_775 ?
C1 W1 C2 75.2(2) 3_775 4_575 ?
C1 W1 C2 132.42(17) . 4_575 ?
C1 W1 C2 132.42(17) 2_755 4_575 ?
C1 W1 C2 75.2(2) 4_575 4_575 ?
C3 W1 C2 136.6(3) . 4_575 ?
C2 W1 C2 86.8(5) 2_755 4_575 ?
C2 W1 C2 58.1(3) . 4_575 ?
C2 W1 C2 58.1(3) 3_775 4_575 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.121(8) . ?
C1 W1 2.169(7) . ?
C2 N2 1.140(11) . ?
C2 W1 2.176(8) . ?
C3 N3 1.114(16) . ?
C3 W1 2.170(11) . ?
C4 O1 1.42(2) . ?
C4 O1 1.42(2) 2_655 ?
C4 O2W 1.520(16) 2_655 ?
C4 H4A 0.9300 . ?
Mn1 O2W 1.84(3) 17_675 ?
Mn1 O2W 1.84(3) . ?
Mn1 N2 2.177(8) . ?
Mn1 N2 2.177(8) 17_675 ?
Mn1 N2 2.177(8) 19 ?
Mn1 N2 2.177(8) 3_675 ?
Mn1 O1 2.32(2) . ?
Mn1 O1 2.32(2) 17_675 ?
Mn2 N3 2.196(11) . ?
Mn2 N1 2.218(6) 27 ?
Mn2 N1 2.218(5) 25_665 ?
Mn2 N1 2.218(5) 26_565 ?
Mn2 N1 2.218(5) 28_655 ?
Mn2 O1W 2.322(9) . ?
N1 Mn2 2.218(5) 25_665 ?
O1 C4 1.42(2) 18_565 ?
O1 H2X 0.8133 . ?
O1 H2Y 0.8133 . ?
O1W H1X 0.8501 . ?
O1W H1Y 0.8501 . ?
O2W C4 1.520(16) 18_565 ?
O2W H2X 0.8499 . ?
O2W H2Y 0.8499 . ?
O3W H3X 0.8499 . ?
O3W H3Y 0.8499 . ?
W1 C1 2.169(7) 3_775 ?
W1 C1 2.169(7) 2_755 ?
W1 C1 2.169(7) 4_575 ?
W1 C2 2.176(8) 2_755 ?
W1 C2 2.176(8) 3_775 ?
W1 C2 2.176(8) 4_575 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C4 O1 Mn1 180.0 2_655 . . . ?
O2W C4 O1 Mn1 180.0 2_655 . . . ?
N2 Mn1 O1 C4 -48.7(2) . . . 18_565 ?
N2 Mn1 O1 C4 131.3(2) 17_675 . . 18_565 ?
N2 Mn1 O1 C4 48.7(2) 19 . . 18_565 ?
N2 Mn1 O1 C4 -131.3(2) 3_675 . . 18_565 ?
N2 Mn1 O1 C4 131.3(2) . . . . ?
N2 Mn1 O1 C4 -48.7(2) 17_675 . . . ?
N2 Mn1 O1 C4 -131.3(2) 19 . . . ?
N2 Mn1 O1 C4 48.7(2) 3_675 . . . ?
N2 Mn1 O2W C4 -48.7(2) . . . 18_565 ?
N2 Mn1 O2W C4 131.3(2) 17_675 . . 18_565 ?
N2 Mn1 O2W C4 48.7(2) 19 . . 18_565 ?
N2 Mn1 O2W C4 -131.3(2) 3_675 . . 18_565 ?
